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目的建立顶空气相色谱法测定盐酸普拉克索中有机溶剂残留量的方法。方法采用Agilent DB-624(30 m×0.25mm,1.4μm)毛细管柱,氮气为载气,程序升温,氢离子火焰检测器,测定盐酸普拉克索中甲醇、异丙醇、乙酸乙酯和四氢呋喃的溶剂残留量。结果甲醇、异丙醇、乙酸乙酯及四氢呋喃色谱峰均能得到有效分离,且质量浓度分别在24.1~96.4mg·L-1、40~160.2mg·L-1、39.9~159.7 mg·L-1和5.8~23.1 mg·L-1内与峰面积呈良好线性关系(r≥0.999 0),平均回收率在93.3%~108.6%内;甲醇、异丙醇、乙酸乙酯和四氢呋喃的检测限分别为0.91、0.6、0.33和0.44 mg·L-1,定量限分别为3.64、2.4、1.33和1.75mg·L-1。结论本方法灵敏、准确、可靠,可用于盐酸普拉克索中残留溶剂的测定。
Objective To establish a method for the determination of residual organic solvents in pramipexole hydrochloride by headspace gas chromatography. Methods The capillary column of Agilent DB-624 (30 m × 0.25 mm, 1.4 μm) was used with nitrogen as the carrier gas, programmed temperature and hydrogen ion flame detector to determine the concentration of methanol, isopropanol, ethyl acetate and tetrahydrofuran in pramipexole hydrochloride Of solvent residue. Results The chromatographic peaks of methanol, isopropanol, ethyl acetate and tetrahydrofuran were effectively separated and the mass concentrations were 24.1-96.4 mg · L-1, 40-160.2 mg · L-1, 39.9-159.7 mg · L- 1 and 5.8 ~ 23.1 mg · L-1 showed good linear relationship with the peak area (r≥0.999 0) and the average recoveries ranged from 93.3% to 108.6%. The detection limits of methanol, isopropanol, ethyl acetate and tetrahydrofuran 0.91, 0.6, 0.33 and 0.44 mg · L-1, respectively. The limits of quantification were 3.64, 2.4, 1.33 and 1.75 mg · L-1, respectively. Conclusion The method is sensitive, accurate and reliable and can be used for the determination of residual solvents in pramipexole hydrochloride.